CN101258857A - Plant tar oil bactericide and preparation thereof - Google Patents
Plant tar oil bactericide and preparation thereof Download PDFInfo
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- CN101258857A CN101258857A CNA2008100708823A CN200810070882A CN101258857A CN 101258857 A CN101258857 A CN 101258857A CN A2008100708823 A CNA2008100708823 A CN A2008100708823A CN 200810070882 A CN200810070882 A CN 200810070882A CN 101258857 A CN101258857 A CN 101258857A
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Abstract
The invention relates to a plant tar bactericide and preparation methods thereof, which comprise a method for preparing a bamboo tat bactericide and a method for preparing a wood tar bactericide. The specific preparation method comprises the steps of extraction, concentration and preparation. The plant tar bactericide of the invention for treating the phytopathogenic bacteria has the advantages of high medical effect, low toxicity, low residue, non-pollution, being no drug resistance and not hurting the natural enemies, etc., and is an environment-friendly bactericide for replacing the traditional antibiotic bactericides and chemically synthesized bactericides.
Description
Technical field
The present invention relates to a kind of bactericide and preparation method thereof, particularly plant species tar oil bactericide and preparation method thereof.
Background technology
The utilization bactericide carries out chemical control to plant disease, has efficient, quick-acting, easy to use, cost performance advantages of higher, and especially before the disease of this season is popular or the popular initial stage, chemical control is the effective way of controlling plant disease.The new type bactericide of developing high-efficiency low-toxicity cheaply always is the hot issue of agriculture field.But along with the enhancing of people's environmental consciousness, the requirement that management is thrown in to new chemical pesticide by government is more and more stricter, and the chemical pesticide development difficulty is very big, expense is high, and success rate is very low.
In China, the medicament of control bacterial diseases of plants mostly is the medicine of various antibioticses, chemosynthesis bactericide, biogenic bactericide etc. greatly.In agricultural production, what the medicament use of control bacterial diseases of plants was maximum is the medicine of various antibioticses, and as agricultural streptomycin, kasugarnycin etc., other is of less types.Because use farm antibiotics to have the healthy and problem such as easily develop immunity to drugs of harm humans, European Union has limited the use of some antibiotics medicaments and has detected in agricultural product in recent years, has influenced the outlet of agricultural products in China greatly.The bactericide of chemosynthesis (comprising bionical bactericide) is big to the interdependency of raw materials for production, equipment, technology, the product price height, and have the production pollution problem.The research and development of other biogenic (as plant resource) bactericide are at present in the positive mushroom development of China, but because the variable factor of biogenic material is too many, really are developed to the bactericide novel form or obtain the novel active presoma and further exploitation is seldom.Therefore, to prevent and treat bacterial disease be the big problem that China is badly in need of solving at present to bacteriostatic material development of new, the non-antibiotic class.
The organic matter that people know some phenols structures has stable bactericidal activity, is applied to the treatment of dermatophyte, bacteriosis and the sterilization of medicine equipment for a long time as phenol, cresol soap, salicylic acid.The Meng Zhao of Qingdao agricultural college gift etc. (Meng Zhaoli. ginkgo and bionical bactericide [M] thereof. Beijing: China Science Tech Publishing House; 2004.) the imitative ginkgol bactericide " Yin Tai " with short-side chain phenol structure (structural formula is a 1-p-hydroxybenzene butanone) of exploitation and " green Supreme Being " (structural formula is adjacent acrylic phenol) be two of China exploitation in recent years efficiently, low toxicity, biodegradable two novel agricultural fungicides, now large-scale production and large tracts of land are promoted the use of.The Li Junqing of Beijing Forestry University etc. disclose a kind of with vegetable tannin by the plant polyphenol that obtains after the hydrogen peroxide oxidation degraded patent (publication number CN1922996A) as agricultural bactericide.Above forefathers' experience shows that the phenols structural material has the potentiality that are developed as bactericide.
Plant tar is vegetable material such as timber, bamboo wood, pass through pyrolysis processing, after collecting the pyroligneous liquor or Bamboo vinegar solution that produces, therefrom isolated thick tar matter, wherein contain a large amount of 2, the 6-syringol, the 4-ethyl-phenol, composition (money China, Zhong Zheke, the Wang Yanbin of phenols structures such as 2-ethyl-phenol, Deng. the GC/M S method of bamboo tar chemical composition is analyzed [J]. bamboo research transactions, 2006,25 (3): 24-27.) (Li Jihong, Lei Tingzhou, Song Huamin, analyze the chemical composition [J] of biomass coke tar Deng the .GC/MS method. Henan science, 2005,23 (1): 41-43.).These materials structurally have similitude with bactericide " Yin Tai " and " green Supreme Being ".Mensuration shows that it has good fungistatic effect equally.
The ability of the height conjugated protein of the aldehydes matter in the plant tar is a principal element of its biocidal property.Tar just shows tangible bacteriostatic activity in very low concentration, and it is by inhibitory enzyme activity, destroys the inhibitory action that the metabolic process of pathogen reaches.In addition, the biocidal property of phenols structure also reaches relevant to the complexing power of metal with the effect of its cell membrane.It can by combine with cell membrane or complexing microorganism living environment in metal ion, destroy the eubolism of pathogen.Number and the numbers of position, side chain, length, kind etc. of the phenolic hydroxyl group of the aldehydes matter in the bamboo tar on phenyl ring can influence its relative toxicity.The aldehydes matter of the complexity in the bamboo tar can make pathogen be difficult for developing immunity to drugs to the common toxicity of pathogen.
Summary of the invention
The purpose of this invention is to provide a kind of environmentally friendly plant tar oil bactericide and preparation method thereof.
The preparation method of plant tar oil bactericide of the present invention comprises the preparation method of bamboo tar oil bactericide and the preparation method of wood tar bactericide, and concrete preparation method comprises extraction, concentrates and preparation.
The preparation method of method one, a kind of bamboo tar oil bactericide may further comprise the steps:
1, extraction: add the organic extractant chloroform in Bamboo vinegar solution, the amount that adds chloroform is 10%～30% (V/V) of Bamboo vinegar solution, 15%～20% (V/V) that optimised quantity is, and the vibration mixing, behind the standing demix, separatory is also collected the bamboo vinegar chloroform extraction liquid of lower floor.Described organic extractant chloroform is liquid, technical pure; Described Bamboo vinegar solution is that market is buied.
2, concentrate: with the chloroform extraction liquid rotary evaporator concentrating under reduced pressure of bamboo vinegar, its vacuum degree control is 0.01MPa, 40～60 ℃ of evaporating temperatures, boil off chloroform after, must bamboo tar standby;
3, preparation: get bamboo tar and mix with organic solvent, be heated to 50～60 ℃ of liquid temperature, stirring and dissolving adds emulsifier again, is the bamboo tar oil bactericide after stirring.The consumption of described bamboo tar, organic solvent and emulsifier accounts for 5%～25% (V/V), 60%～90% (V/V) and 5%～15% (V/V) of bamboo tar oil bactericide respectively; Described organic solvent is dimethyl formamide or ethanol or acetone; Described emulsifier is Tween-80 or farming breast 0206.Organic solvent and emulsifier are liquid, technical pure.During actual production, generally get 1/2 of organic solvent total amount, being heated to the liquid temperature is 50～60 ℃, and stirring and dissolving behind the adding bamboo tar adds emulsifier for mixing again, adds the surplus organic solvent and stirs, and is the bamboo tar oil bactericide.
The preparation method of method two, a kind of wood tar bactericide may further comprise the steps:
1, extraction: add the organic extractant chloroform in pyroligneous liquor, the amount that adds chloroform is 10%～30% (V/V) of pyroligneous liquor, optimised quantity be 15%～20%, the vibration mixing, behind the standing demix, separatory is also collected the wooden vinegar chloroform extraction liquid of lower floor; Described organic extractant chloroform is liquid, technical pure; Described pyroligneous liquor is that market is buied.
2, concentrate: with the chloroform extraction liquid rotary evaporator concentrating under reduced pressure of wooden vinegar, its vacuum degree control is 0.01MPa, 40～60 ℃ of evaporating temperatures, boil off chloroform after, must wood tar standby.
3, preparation: get wood tar and mix with organic solvent, be heated to 50～60 ℃ of liquid temperature, stirring and dissolving adds emulsifier again, and stirring is the wood tar bactericide.The consumption of described wood tar, organic solvent and emulsifier accounts for 5%～25% (V/V), 60%～90% (V/V), 5%～15% (V/V) of wood tar bactericide respectively; Described organic solvent is dimethyl formamide or ethanol or acetone; Described emulsifier is Tween-80 or farming breast 0206.Organic solvent and emulsifier are liquid, technical pure.During actual production, generally get 1/2 of organic solvent total amount, being heated to the liquid temperature is 50～60 ℃, and stirring and dissolving behind the adding wood tar adds emulsifier for mixing again, adds the surplus organic solvent and stirs, and is the wood tar bactericide.
Plant tar oil bactericide of the present invention has good control efficiency to c itrus canker germ (Xanthomonascampestris pv.citri), tomato ralstonia solanacearum (Ralstonia solanacearum), cabbage black rot bacterium (Xanthomonas campestris pv.campestris), bacterial spot of tomato bacterium (Pseudomonas syingae pv.tomato), the bacillary fruit spot germ of watermelon bacterial diseases of plants such as (Acidovorax avenae subsp.citrulli).
Plant tar oil bactericide of the present invention, not only has the effect that suppresses pathogenetic bacteria, mould, fungi, yeast and virus etc. had resistance of wide spectrum in interior microorganism, simultaneously some insects are had avoidance effect, a small amount of pyroligneous liquor that is wherein contained or Bamboo vinegar solution promote the healthy and strong growth of plant in addition, strengthen the function of resistance against diseases.Specifically, plant tar oil bactericide of the present invention has the effect of kinds of protect plant concurrently in case the indigenous bacteria of curing the disease is main.
Plant tar oil bactericide of the present invention, have high-drug-effect, low toxicity, low-residual, nuisanceless, the target germ is not developed immunity to drugs and is not injured advantages such as natural enemy, alternative traditional antibiotics bactericide, chemosynthesis bactericide.
Plant tar oil bactericide of the present invention has the stability of ultraviolet light, heat, storage, soda acid.
Embodiment
In order fully to disclose plant species tar oil bactericide of the present invention and preparation method thereof, be illustrated below in conjunction with embodiment.
1: one plant species tar oil bactericide of embodiment---the preparation method of bamboo tar oil bactericide
Put Bamboo vinegar solution in separatory funnel, add the organic extractant chloroform again, the chloroform amount of adding is 15% (V/V) of Bamboo vinegar solution, the vibration mixing, and behind the standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively; Add chloroform once more in the water layer of collecting, addition is 15% (V/V) of Bamboo vinegar solution, oscillation extraction, and behind the standing demix, the water layer above collecting respectively and the chloroform extraction liquid of lower floor; So re-extract is 3 times; The combined chloroform extract.With chloroform extraction liquid rotary evaporator concentrating under reduced pressure, wherein vacuum degree control is 0.01MPa, and 50 ℃ of evaporating temperatures boil off chloroform, gets bamboo tar.Get bamboo tar and mix with ethanol, be heated to 55 ℃ of liquid temperature, stirring and dissolving adds Tween-80 again, and stirring is the bamboo tar oil bactericide.The consumption of described bamboo tar, ethanol and Tween-80 accounts for 20% (V/V), 70% (V/V), 10% (V/V) of bamboo tar oil bactericide respectively.
2: one plant species tar oil bactericides of embodiment---the preparation method of wood tar bactericide
Put pyroligneous liquor in separatory funnel, add the organic extractant chloroform again, the chloroform amount of adding is 20% (V/V) of pyroligneous liquor, the vibration mixing, and behind the standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively.Add chloroform in the water layer of collecting, addition is 20% (V/V) of pyroligneous liquor, with above-mentioned method extraction, and the water layer above collecting respectively and the chloroform extraction liquid of lower floor.So re-extract is 3 times.The combined chloroform extract.With chloroform extraction liquid rotary evaporator concentrating under reduced pressure, wherein vacuum degree control is 0.01MPa, and 55 ℃ of evaporating temperatures boil off chloroform, gets wood tar.Get wood tar and mix with acetone, be heated to 50 ℃ of liquid temperature, stirring and dissolving adds farming breast 0206 again, and stirring is the wood tar bactericide.The consumption of described wood tar, acetone and farming breast 0206 accounts for 10% (V/V), 75% (V/V), 15% (V/V) of wood tar bactericide respectively.
Below be example with a kind of bamboo tar oil bactericide of the present invention, the bactericidal effect of plant tar oil bactericide of the present invention is described.
1, a kind of bamboo tar oil bactericide is measured the bactericidal effect of specific pathogen bacterium
Adopt inhibition zone method, verify the bactericidal effect of bamboo tar oil bactericide of the present invention 8 plant species pathogenetic bacterias such as c itrus canker germ, tomato ralstonia solanacearum, paddy bacterial slice germ, Xanthomonas oryzae, cabbage black rot bacterium, tomato bacterial spot germ, the bacillary fruit spot germ of watermelon, corn bacterial striped germs.
Preparation for the examination bacterial suspension: will be seeded under the aseptic condition on the test tube slant medium respectively for the examination bacterial classification, place in 37 ℃ of constant incubators and cultivated 24-36 hour, behind the basicly stable bacterium colony of size to be formed, add the 3ml sterile water, vibrated 1 minute, and formed suspension bacteria liquid.
With NA medium heat fused.Add the 0.1ml suspension bacteria liquid in the 9cm sterile petri dish, the NA medium that is chilled to 45～50 ℃ with 20ml mixes.Contain medicine hole (do not wear the end to ware at the bottom of) with the 9mm card punch getting on the culture medium flat plate.The implantation concentration dilution is 1% bamboo tar oil bactericide 0.05ml of the present invention respectively in containing the medicine hole.Be provided with in the same old way, and repeat ten times.Place 37 ℃ of insulating boxs to cultivate 24 hours, measure the inhibition zone size of bamboo tar oil bactericide of the present invention, calculating mean value every kind of bacterial strain.Bamboo tar oil bactericide of the present invention is as shown in table 1 to the bactericidal effect of specific pathogen bacterium.
Table 1 bamboo tar oil bactericide is to the bactericidal effect of specific pathogen bacterium
The criterion of reference drug sensitive experiment is Gao Min at inhibition zone greater than 9mm, illustrate bamboo tar oil bactericide of the present invention to prevent and treat c itrus canker germ, tomato ralstonia solanacearum, cabbage black rot bacterium, tomato fruit spot germ, watermelon fruit spot germ equivalence fruit is fine.
2, the bamboo tar oil bactericide is to the sterilization toxicity test of specific pathogen bacterium
With c itrus canker germ, tomato ralstonia solanacearum, cabbage black rot bacterium, tomato spot germ, watermelon fruit spot germ etc. serves as for the examination bacterium, adopts the method for plate culture count, investigates the bacteriostasis rate of variable concentrations bamboo tar oil bactericide of the present invention.
Bamboo tar oil bactericide of the present invention is diluted to the medicament of 5 concentration gradients.
To add the sterile water of 3ml for the examination bacterium after cultivating 24～48h (28 ℃) on the NA slant medium, the vibration mixing is made bacterial suspension, is diluted to 10 with sterile water
2CFU/ml, drawing 1ml from dilute the back bacteria suspension is in the culture dish of 9cm to diameter, add the NA medium (45～50 ℃) of 1ml dilution for certain density medicament and 8ml, abundant mixing, make bacterium medicine medium, under 28 ℃ of constant temperature, cultivate 24-48h, observe single clump count of each processing of statistics.Each drug concentration is provided with 5 repetitions.Result such as table 2.
Table 2 bamboo tar oil bactericide of the present invention is to the sterilization virulence of specific pathogen bacterium
Claims (6)
1, a kind of preparation method of bamboo tar oil bactericide is characterized in that may further comprise the steps:
(1) extraction: add the organic extractant chloroform in Bamboo vinegar solution, the amount that adds chloroform is 10%～30% of a Bamboo vinegar solution, optimised quantity be 15%～20%, the vibration mixing, behind the standing demix, separatory is also collected the bamboo vinegar chloroform extraction liquid of lower floor;
(2) concentrate: with the chloroform extraction liquid rotary evaporator concentrating under reduced pressure of bamboo vinegar, its vacuum degree control is 0.01MPa, 40～60 ℃ of evaporating temperatures, boil off chloroform after, must bamboo tar standby;
(3) preparation: get bamboo tar and mix with organic solvent, be heated to 50～60 ℃ of liquid temperature, stirring and dissolving adds emulsifier again, is the bamboo tar oil bactericide after stirring.The consumption of described bamboo tar, organic solvent and emulsifier accounts for 5%～25%, 60%～90% and 5%～15% of bamboo tar oil bactericide respectively;
2, the preparation method of a kind of bamboo tar oil bactericide according to claim 1 and 2 is characterized in that described extraction, and behind standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively; Add chloroform once more in the water layer of collecting, addition is 15% of a Bamboo vinegar solution, the vibration mixing, and behind the standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively; So re-extract is 3 times; The combined chloroform extract.
3, the bamboo tar oil bactericide for preparing by claim 1 or 2 described methods.
4, a kind of preparation method of wood tar bactericide is characterized in that may further comprise the steps:
(1) extraction: add the organic extractant chloroform in pyroligneous liquor, the amount that adds chloroform is 10%～30% of a pyroligneous liquor, optimised quantity be 15%～20%, the vibration mixing, behind the standing demix, separatory is also collected the wooden vinegar chloroform extraction liquid of lower floor;
(2) concentrate: with the chloroform extraction liquid rotary evaporator concentrating under reduced pressure of wooden vinegar, its vacuum degree control is 0.01MPa, 40～60 ℃ of evaporating temperatures, boil off chloroform after, must wood tar standby;
(3) preparation: get wood tar and mix with organic solvent, be heated to 50～60 ℃ of liquid temperature, stirring and dissolving adds emulsifier again, and stirring is the wood tar bactericide; The consumption of described wood tar, organic solvent and emulsifier accounts for 5%～25%, 60%～90%, 5%～15% of wood tar bactericide respectively.
5, according to the preparation method of claim 5 or 6 described a kind of wood tar bactericides, it is characterized in that described extraction, behind standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively; Add chloroform once more in the water layer of collecting, addition is 15% of a pyroligneous liquor, the vibration mixing, and behind the standing demix, separatory is also collected the top water layer and the chloroform extraction liquid of lower floor respectively; So re-extract is 3 times; The combined chloroform extract.
6, the wood tar bactericide for preparing by claim 4 or 5 described methods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2008100708823A CN101258857A (en) | 2008-04-11 | 2008-04-11 | Plant tar oil bactericide and preparation thereof |
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| CNA2008100708823A CN101258857A (en) | 2008-04-11 | 2008-04-11 | Plant tar oil bactericide and preparation thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102499266A (en) * | 2011-10-25 | 2012-06-20 | 广州迪森热能技术股份有限公司 | Water-soluble wood tar composite disinfectant |
| CN105594764A (en) * | 2015-12-25 | 2016-05-25 | 郑州金土地能源科技有限公司 | Plant insecticide |
| CN105638737A (en) * | 2016-01-25 | 2016-06-08 | 抚顺市世纪东方生物质综合技术开发有限公司 | Mongolian oak wood vinegar extract, preparation method and application thereof and harmless insecticide |
| CN105685102A (en) * | 2015-12-26 | 2016-06-22 | 郑州金土地能源科技有限公司 | Environment-friendly sterilization insect repellant containing wood tar |
| CN106561713A (en) * | 2016-10-09 | 2017-04-19 | 西南大学 | Method for preventing and treating green spot of citruses by using wood vinegar |
| CN106665657A (en) * | 2015-11-11 | 2017-05-17 | 孙德玉 | Compound disinfection agent and preparation method thereof |
| CN107232232A (en) * | 2017-07-07 | 2017-10-10 | 浙江农林大学 | A kind of bamboo tar is the natural herbicide and its manufacture method of active component |
| CN107296060A (en) * | 2017-07-07 | 2017-10-27 | 浙江农林大学 | A kind of natural herbicide and its manufacture method containing wood tar |
-
2008
- 2008-04-11 CN CNA2008100708823A patent/CN101258857A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102499266A (en) * | 2011-10-25 | 2012-06-20 | 广州迪森热能技术股份有限公司 | Water-soluble wood tar composite disinfectant |
| CN106665657A (en) * | 2015-11-11 | 2017-05-17 | 孙德玉 | Compound disinfection agent and preparation method thereof |
| CN105594764A (en) * | 2015-12-25 | 2016-05-25 | 郑州金土地能源科技有限公司 | Plant insecticide |
| CN105685102A (en) * | 2015-12-26 | 2016-06-22 | 郑州金土地能源科技有限公司 | Environment-friendly sterilization insect repellant containing wood tar |
| CN105638737A (en) * | 2016-01-25 | 2016-06-08 | 抚顺市世纪东方生物质综合技术开发有限公司 | Mongolian oak wood vinegar extract, preparation method and application thereof and harmless insecticide |
| CN105638737B (en) * | 2016-01-25 | 2018-08-14 | 抚顺市世纪东方生物质综合技术开发有限公司 | Toothed oak wood wood vinegar extract and its preparation method and application and environmental-pollution insecticide |
| CN106561713A (en) * | 2016-10-09 | 2017-04-19 | 西南大学 | Method for preventing and treating green spot of citruses by using wood vinegar |
| CN106561713B (en) * | 2016-10-09 | 2018-11-20 | 西南大学 | Using the method for wood vinegar prevention and treatment citrus paper disk test |
| CN107232232A (en) * | 2017-07-07 | 2017-10-10 | 浙江农林大学 | A kind of bamboo tar is the natural herbicide and its manufacture method of active component |
| CN107296060A (en) * | 2017-07-07 | 2017-10-27 | 浙江农林大学 | A kind of natural herbicide and its manufacture method containing wood tar |
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